Gas purification



2 Sheets-Sheet l H. H. DOW

GAS PURIFICATION Filed May 25, 1928 L 1U ,EE @dini ,mi nlm-- Juy 25, 1933.

A TTORNEYS July 25, 1933. H. H. Dow 1,919,778

GAS PURIFICATION Filed May 25, 1928 2 Sheets-Sheet 2 I N VEN TOR.

'gefefm 00W Patented July 25, 1933 'Um-TED I STATES PATENT OFFICE y. HERBERT II. Dow, or MIDLAND, MICHIGAN, AssIGNoR rro THE Dow CHEMICAL CoM.

PANY, or MIDLAND, MICHIGAN, A CORPORATION or MICHIGAN GAS rURIFICA'rIoN of alkaliv metal hydroxides to purify the hydrogen-nitrogen gas mixture used in the syn- 755 thetic ammonia process. Before purification thehydrogen-nitrogen. gas mixture usually contains water vapor, carbonl dioxide and/or other gaseous constituents which act to re'- o duce the efficacy of the catalyst and theconheretofore to purify the gas mixture is the process of scrubbing with liquid ammonia,v

another being that of scrubbing with aqueous caustic soda. While the 4vaqueous caustic Soda scrubbino` removes a large portion of the objectionable gases still it leaves vmoisi ture in the reaction mixture which is objectionableg' I have discovered anefficientgas purifi-V cation ymethod which utilizes coating the inner or contained surfaces of ay gas purification chambcrwith anhydrous or near anhydrous alkali and then recoating same when the alkali thereon becomes spent, said coating being accomplished without introducing into the purifierorinto'the circulatory system, air or foreign gasor vapor of any kind. To the accomplishment ofthe foregoing and related l ends, the inventionthen consists of thev steps. and means hereinafter fully described and particularly pointed out in the claims, `the annexed drawingsand the following description setting forth in detail certain lmeans and modesof carrying out they invention,` such `.disclosed means and modes illustrating,showever, but several of the various ways in which the principle of they invention ,may be used. y Y

InV said annexed Y drawings 4 Fig. 1 Ashows in crossv section one type of apparatus particularly adapted for use .in

this invention. f f o v i Fig .2 shows the gas puriiierjin further detail..` if .i

Fig. 1 shows two gas purifiers, or4 part of a seriesof purifiers, which are so connected.

that they can Vbe used one, at atime, or in series or in parallel.. vGras purifier or vessel l (whichlis a duplicateof 1) contains a suitable filling material-'2,such as meta-l rings,

Application filed May 23,

version ehiciency. Among methods used 1928. Serial N0. 279,95L`

which VAmay be placed systematically or dumped in heterogeneously. Partition 5 dir vides the purifier chamber into two sections so that the gas, connections are all on the top of the purifier and a relatively long path made for the gas being purified. Perforated plate `or grating 14 acts as a support for lthe filling material and allows free'passage. of the gas around the end'of partition 5.

In order to present as much purifying surface as possible to the-gases being purified, the purifiers ywill ordinarily be hooked up in series, for instance, byhaving valves 4, 6 and 7 open and avalves, 5 and 8 closed, .they gas flow will be from raw gasv main 2l vthrough valve 4 .into purifier l, around partition 5 and thence through valve 6 to purifier l and around partition, 5 andv thence through valve 7 to the purified gas main'20. l

When the alkali coating in one of the purifiers, usually the first one of the series, be-

comes inefficient as may be determined in'any.

well known manner,this purifier is cut out of the ,circuit for recoatingwhile the gas to be` source is then forced intopurifier l in any,

Convenient manner through pipe 22 and valve l5 until the purifier is substantially full as may be determined `in any'well iknown manner. Y Valve 1l is then closed and the molten alkali allowed to drain throughvalve e 15 and pipe 22 to a suitable receiver. A modification of this procedure is to leave lvalve 11 .open and allow-the molten alkali to overfiow therethrough and thus flush away the impurities V.in the purifier, following which valve l1 isclosed` and the` remaining molten alkali allowed -to drain-back'through l valve ljand pipe 22 asA described above. i

When ,starting kto drain the moltenjalkali through valve l5 and pipe 22 in eithercase,v valve 3 ori,y is cracked sothat the purifier is filled with gas as fast as the molten alkali is withdrawn. Purifier 1 is then ready to be hooked into the circuit and is preferably so vconnected in the series that the gases being alkali, and also as an equalizer and overflow for the alkali when flushing away impurities, may be of any suitable construction, one type of which is illustrated.

The purifier is packed at 13 or in any convenient manner so as to make it satisfactorily gas tight under operating conditions.

A modification of the purifiers illustrated in Fig. 1 can be made by extending one of the gas connecting pipes Vto the space below perforatedplate or grating 14 which will lthus eliminate the necessity of partition 5.

The purifier is preferably made of such form and construction as to :facilitate recoating with alkali as well as to operate under the same pressure as utilized in the ammonia producing apparatus. When operating under this high'pressure the handling` of the raw gases tothe purifier and thence to the ammonia producing apparatus is notv only simplifiedbut incidentally accomplishes better absorption of impurities than Ais possible under lower pressures.

The above described methods of recoating or regenerating; the activity of the spent alka# li, which may be either caustic soda, caustic potash or a mixture of the two, has theadvantage of avoiding entrance into the sys-l tem of air or other objectionable gases. If the chamber were to be opened to the air for removing spent alkali and recharging with broken, flaked or granulated alkali in any manner such as on trays, or as packing, air'would be taken intothe purifier" and it wouldlater be necessary to wash that air out with gases fromy the system, venting same to waste until the contaminating gas was re moved.

While my `invention can be used as the only purification for thev raw gases used to produce synthetic ammonia, still it `can in some cases be used to better advantage if the raw gases are given a preliminary washing suchas with water or cuprous solution or both.

While either caustic soda or caustic 'potash can be used in this process I prefer to use a mixture of the two which operates satisfactorily and has a lower freezing point kthan either of the alkalis above. When employing alkali mixtures I prefer to use the mixture having the lowest melting point.

This mixture which is commonly known as the eutectic mixture contains approximately 46.9 per cent of potassium hydroxide and has a melting point of approximately 185 C. The use of mixtures in itself allows the coat ing 'of the purifier elements to be handled at a relatively low temperature which from the standpoint of operation is desirable.

In order to minimize the difficulties encountered in handling molten alkali, as are well known to those versed in the art, each purifier is preferably provided with a jacket 23 which may be supplied with heat in any suitablemanner such as for instance stack gases from the furnace which supplies heat for melting the alkali. This same jacket can also be used to cool the purifier as needed by passing therethrough cold air or other suitable cooling iiuid. Likewise all pipes carrying the molten alkali are suitably lagged to prevent freezing during the alkali coating process. l

While I have described my invention'in terms of purifying hydrogen-nitrogen, gas mixtures used in producing syntheticV ammonia, I do not wish to be limited to that particular field as my'invention is equally applicable to purifying any gas or gas mixture that may be purified by treatment with caustic soda, caustic potash or a mixture of the two. Other modes of applying the principle of my invention may be employed instead of those explained, change being made as regards the method herein disclosed, provided the step or steps stated by any of the following claims or the equivalent of such step or steps be employed.

I thereforeparticularly point out and dis-v tinctly claim as my invention 1. In a method of purifying a gas by contact with alkali, the steps which consist in substantially flooding the .surface within a suitable vessel with alkali metal hydroxide by substantially filling said vessel with molten alkali and then withdrawing excess of same while admitting the gas being puried, whereby said surface is ,coated with alkali and the excess thereof removed without introducing gas other than that being purified.

2. In amethod of purifying a gas by contact with alkali, the steps which consist in coating a substantial portiony of the surface within a suitable vessel with a mixture of caustic soda and caustic potash by substantially filling said vessel with saidalkali mixture in molten condition and then withdrawing excess of same while admitting the gas being purified, whereby said surface is coated with alkali andthe excess thereof removed without introducingigas other,` than that being purified. i

3. In a method of purifying a gas by contact with alkali, the steps which consist in coating substantially all of the contained surfaces in a suitable pressure vessel with alkali metal hydroxide by filling said vessel with molten alkali and then withdrawing excess of same while admitting the gas being purified, whereby said surfaces are coated with alkali and the excess thereof removed without introducing gas other than that being purified.

4. In a method of purifying a hydrogennitrogen gas mixture by Contact with alkali, the steps which consist in coating substantially all of the surfaces within a suitable Vessel with alkali metal hydroxide by substantially filling said vessel with molten alkali and then withdrawing excess of same While admitting the gas being purified,

whereby said surfaces are coated with alkali and the excessy thereof removed without intr'oducing'gas other than that being purified.

5. In :a method of purifying a hydrogennitrogen gas mixture by Contact with alkali,v

the steps which consist in coating substantially all of the surfaces within a suitablev vessel with. a mixture of caustic soda and caustic potash by substantially filling said vessel with said alkali mixture in molten'condition and then withdrawing excessv of same' vwhile admitting the said gas mixture, .whereby said surfaces are coated with alkali 4and thek excess thereof removed without introducing other gas.

f HERBERTH. DOW. v 

